JP2012048767A - Soft magnetic alloy for magnetic recording medium, sputtering target material and magnetic recording medium - Google Patents
Soft magnetic alloy for magnetic recording medium, sputtering target material and magnetic recording medium Download PDFInfo
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- 230000005291 magnetic effect Effects 0.000 title claims abstract description 57
- 229910001004 magnetic alloy Inorganic materials 0.000 title claims abstract description 19
- 238000005477 sputtering target Methods 0.000 title claims abstract description 13
- 239000013077 target material Substances 0.000 title claims abstract description 9
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 10
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 229910052715 tantalum Inorganic materials 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 abstract description 12
- 239000000956 alloy Substances 0.000 abstract description 12
- 239000010409 thin film Substances 0.000 abstract description 6
- 230000004907 flux Effects 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 239000010408 film Substances 0.000 description 9
- 238000011156 evaluation Methods 0.000 description 7
- 238000010791 quenching Methods 0.000 description 7
- 230000000171 quenching effect Effects 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 125000001475 halogen functional group Chemical group 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 229910000521 B alloy Inorganic materials 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/64—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent
- G11B5/65—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition
- G11B5/657—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition containing inorganic, non-oxide compound of Si, N, P, B, H or C, e.g. in metal alloy or compound
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/64—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent
- G11B5/66—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent the record carriers consisting of several layers
- G11B5/667—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent the record carriers consisting of several layers including a soft magnetic layer
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
- G11B5/851—Coating a support with a magnetic layer by sputtering
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
- Thin Magnetic Films (AREA)
- Magnetic Record Carriers (AREA)
- Soft Magnetic Materials (AREA)
Abstract
Description
本発明は、垂直磁気記録媒体における軟磁性層膜として用いるＣｏ−（Ｚｒ，Ｈｆ）−Ｂ系合金およびスパッタリングターゲット材並びに磁気記録媒体に関するものである。 The present invention relates to a Co— (Zr, Hf) —B alloy used as a soft magnetic layer film in a perpendicular magnetic recording medium, a sputtering target material, and a magnetic recording medium.
近年、磁気記録技術の進歩は著しく、ドライブの大容量化のために、磁気記録媒体の高記録密度化が進められており、従来普及していた面内磁気記録媒体より更に高記録密度が実現できる、垂直磁気記録方式が実用化されている。ここで垂直磁気記録方式とは、垂直磁気記録媒体の磁性膜中の媒体面に対して磁化容易軸が垂直方向に配向するように形成したものであり、高記録密度に適した方法である。そして、垂直磁気記録方式においては、記録感度を高めた磁気記録膜層と軟磁性膜層とを有する２層記録媒体が開発されている。この磁気記録膜層には一般的にＣｏＣｒＰｔ−ＳｉＯ2 系合金が用いられている。 In recent years, the magnetic recording technology has been remarkably advanced, and the recording density of magnetic recording media has been increased to increase the capacity of the drive, realizing a higher recording density than the conventional in-plane magnetic recording media. A perpendicular magnetic recording system capable of being used has been put into practical use. Here, the perpendicular magnetic recording method is a method suitable for high recording density, in which the easy axis of magnetization is oriented perpendicularly to the medium surface in the magnetic film of the perpendicular magnetic recording medium. In the perpendicular magnetic recording system, a two-layer recording medium having a magnetic recording film layer and a soft magnetic film layer with improved recording sensitivity has been developed. A CoCrPt—SiO 2 alloy is generally used for the magnetic recording film layer.
一方、従来の軟磁性膜層には、強磁性と非晶質性が必要であり、さらに垂直磁気記録媒体の用途や使用環境によっては、高飽和磁束密度、高耐食性、高硬度など様々な特性が付加的に要求される。例えば特開２００８−２６０９７０号公報（特許文献１）に開示されているように、耐食性の高い強磁性元素であるＣｏをベースとし、非晶質性を高めるためにＺｒをはじめとした非晶質化促進元素が添加されたものが用いられている。 On the other hand, conventional soft magnetic film layers need to be ferromagnetic and amorphous, and various properties such as high saturation magnetic flux density, high corrosion resistance, and high hardness depend on the application and usage environment of perpendicular magnetic recording media. Is additionally required. For example, as disclosed in Japanese Patent Application Laid-Open No. 2008-260970 (Patent Document 1), an amorphous material including Co, which is a ferromagnetic element having high corrosion resistance, and Zr in order to enhance the amorphous property. A material to which a chemical conversion promoting element is added is used.
また、特開２００８−２９９９０５号公報（特許文献２）に開示されているように、Ｆｅを添加することにより高い飽和磁束密度を得ており、Ｂを添加することにより高い硬度を得ている。更に近年では、従来から要求されてきた上記特性のほか、低い保磁力を有する軟磁性膜用合金が要求されるようになってきた。
上述したような課題を解決するために、発明者らは垂直磁気記録媒体の軟磁性膜用合金の保磁力に及ぼす合金元素の影響について詳細に検討した結果、Ｚｒ，Ｈｆ，Ｂ量を適正な範囲とすることで、垂直磁気記録媒体用の低保磁力軟磁性合金が得られることを見出した。さらに、現在、垂直磁気記録媒体用軟磁性合金は、高い飽和磁束密度を得るための元素として、Ｆｅを２５％から６０％近くまで含むものが主流として用いられていることから、必須元素としてＦｅが多用されてきたが、このＦｅ添加が保磁力を大幅に増大させてしまうことを見出した。これらを考慮し発明した低い保磁力を有する垂直磁気記録媒体用軟磁性合金およびこの合金の薄膜を作製するためのスパッタリングターゲットを提供するものである。 In order to solve the above-described problems, the inventors have studied in detail the influence of the alloy element on the coercive force of the soft magnetic film alloy of the perpendicular magnetic recording medium. As a result, the Zr, Hf, and B amounts are appropriately set. It was found that a low coercive force soft magnetic alloy for perpendicular magnetic recording media can be obtained by setting the range. Furthermore, at present, soft magnetic alloys for perpendicular magnetic recording media are mainly used as elements for obtaining a high saturation magnetic flux density, and those containing Fe from 25% to nearly 60% are mainly used. However, it has been found that the addition of Fe greatly increases the coercive force. The present invention provides a soft magnetic alloy for a perpendicular magnetic recording medium having a low coercive force invented in consideration of the above, and a sputtering target for producing a thin film of this alloy.
その発明の要旨とするところは、
（１）ａｔ．％で、Ｚｒ，Ｈｆの１種または２種を合計で６〜２０％、Ｂを１〜２０％含み、残部Ｃｏおよび不可避的不純物よりなり、かつ式（１）を満たすことを特徴とする磁気記録媒体用軟磁性合金。
６≦２×（Ｚｒ％＋Ｈｆ％）−Ｂ％≦１６ … （１）
（２）請求項１に記載の磁気記録媒体用軟磁性合金において、Ｆｅ添加され、その添加量が式（２）を満たすことを特徴とする磁気記録媒体用軟磁性合金。
Ｆｅ％／（Ｆｅ％＋Ｃｏ％）＜０．２０ … （２）
（３）Ｔｉ，Ｖ，Ｎｂ，Ｔａ，Ｃｒ，Ｍｏ，Ｗ，Ｎｉ，Ａｌ，Ｓｉ，Ｐの１種または２種以上を合計７％以下添加したことを特徴とする前記（１）または（２）に記載の磁気記録媒体用軟磁性合金。
（４）前記（１）〜（３）のいずれか１項に記載の磁気記録媒体用軟磁性合金を用いたスパッタリングターゲット材。
（５）前記（１）〜（３）のいずれか１項に記載の磁気記録媒体用軟磁性合金を用いた磁気記録媒体にある。
The gist of the invention is that
(1) at. %, One or two of Zr and Hf in total 6 to 20%, B 1 to 20%, the balance being Co and inevitable impurities, and satisfying the formula (1) Soft magnetic alloy for recording media.
6 ≦ 2 × (Zr% + Hf%) − B% ≦ 16 (1)
(2) A soft magnetic alloy for a magnetic recording medium according to claim 1, wherein Fe is added and the addition amount satisfies the formula (2).
Fe% / (Fe% + Co%) <0.20 (2)
(3) One or more of Ti, V, Nb, Ta, Cr, Mo, W, Ni, Al, Si, and P are added in a total of 7% or less. (1) or (2 The soft magnetic alloy for magnetic recording media as described in 1).
(4) A sputtering target material using the soft magnetic alloy for magnetic recording media according to any one of (1) to (3).
(5) A magnetic recording medium using the soft magnetic alloy for a magnetic recording medium according to any one of (1) to (3).
以上述べたように、本発明により低い保磁力、高非晶質性、高耐食性および高硬度を有する垂直磁気記録媒体用軟磁性合金およびこの合金の薄膜を作製するためのスパッタリングターゲットを提供するものである。 As described above, the present invention provides a soft magnetic alloy for perpendicular magnetic recording media having low coercivity, high amorphousness, high corrosion resistance and high hardness, and a sputtering target for producing a thin film of this alloy. It is.
以下、本発明に限定した理由を述べる。
Ｚｒ，Ｈｆの１種または２種を合計で６〜２０％
本合金においてＺｒおよびＨｆは非晶質性を改善する効果があるとともに、Ｂ添加量との相関を最適化することにより、低い保磁力を得るための必須元素であり、６％未満では十分な非晶質性、低保磁力が得られず、また、２０％を超えると十分な飽和磁束密度が得られないことから、その範囲を６〜２０％とした。好ましくは１０〜１５％とする。
Hereinafter, the reason limited to the present invention will be described.
6 to 20% in total of one or two of Zr and Hf
In this alloy, Zr and Hf have the effect of improving the amorphousness, and are the essential elements for obtaining a low coercive force by optimizing the correlation with the B addition amount. Amorphous and low coercive force cannot be obtained, and if it exceeds 20%, a sufficient saturation magnetic flux density cannot be obtained, so the range was made 6 to 20%. Preferably it is 10 to 15%.
Ｂを１〜２０％
本合金においてＢは非晶質性を改善する効果があるとともに、ＺｒやＨｆの添加量との相関を最適化することにより、低い保磁力を得るための必須元素である。Ｂ添加量が１％未満では十分な非晶質性、低保磁力が得られず、２０％を超えると十分な飽和磁束密度が得られない。また、Ｂは硬度を増大させる効果も有することから、その範囲を１〜２０％とした。好ましくは５〜１５％とする。
1-20% of B
In this alloy, B is an essential element for obtaining a low coercive force by optimizing the correlation with the addition amount of Zr and Hf as well as having an effect of improving the amorphousness. If the amount of B added is less than 1%, sufficient amorphousness and low coercive force cannot be obtained, and if it exceeds 20%, sufficient saturation magnetic flux density cannot be obtained. Moreover, since B also has an effect of increasing the hardness, the range is set to 1 to 20%. Preferably it is 5 to 15%.
６≦２×（Ｚｒ％＋Ｈｆ％）−Ｂ％≦１６ … （１）
Ｚｒ，Ｈｆ，Ｂ添加量を式（１）の範囲とすることにより、低い保磁力が得られる。この範囲外では保磁力が増大してしまう。好ましくは、８≦２×（Ｚｒ％＋Ｈｆ％）−Ｂ％≦１４、より好ましくは９≦２×（Ｚｒ％＋Ｈｆ％）−Ｂ％≦１２である。これらは保磁力に及ぼす添加元素の影響を詳細に検討し、Ｚｒ％＋Ｈｆ％の添加量の２倍にしたがってＢの添加量を増加させていくことにより、低い保磁力を示す領域があることを明らかにした結果、得られた式である。
6 ≦ 2 × (Zr% + Hf%) − B% ≦ 16 (1)
A low coercive force can be obtained by setting the amount of Zr, Hf, and B added in the range of the formula (1). Outside this range, the coercive force increases. Preferably, 8 ≦ 2 × (Zr% + Hf%) − B% ≦ 14, more preferably 9 ≦ 2 × (Zr% + Hf%) − B% ≦ 12. In these studies, the influence of the additive element on the coercive force is examined in detail, and there is a region showing a low coercive force by increasing the additive amount of B according to twice the additive amount of Zr% + Hf%. As a result of clarification, this is the formula obtained.
Ｆｅ％／（Ｆｅ％＋Ｃｏ％）＜０．２０ … （２）
本合金においてＦｅは飽和磁束密度を増加させる効果があるが、式（２）の割合を超えて添加すると保磁力を増大させてしまう。好ましくはＦｅ％／（Ｆｅ％＋Ｃｏ％）＜０．１０、より好ましくはＦｅ％／（Ｆｅ％＋Ｃｏ％）＜０．０５、更に好ましくはＦｅ無添加である。
Fe% / (Fe% + Co%) <0.20 (2)
In this alloy, Fe has an effect of increasing the saturation magnetic flux density, but if added exceeding the ratio of the formula (2), the coercive force is increased. Preferably, Fe% / (Fe% + Co%) <0.10, more preferably Fe% / (Fe% + Co%) <0.05, and even more preferably no Fe added.
Ｔｉ，Ｖ，Ｎｂ，Ｔａ，Ｃｒ，Ｍｏ，Ｗ，Ｎｉ，Ａｌ，Ｓｉ，Ｐの１種または２種以上を合計７％以下添加
本合金において、Ｔｉ，Ｖ，Ｎｂ，Ｔａ，Ｃｒ，Ｍｏ，Ｗ，Ｎｉ，Ａｌ，Ｓｉ，Ｐはいずれも僅かではあるが保磁力を下げる効果がある。しかしながら、７％を超えて添加すると飽和磁束密度が低下することから、その上限を７％とした。
Add one or more of Ti, V, Nb, Ta, Cr, Mo, W, Ni, Al, Si, P to a total of 7% or less. In this alloy, Ti, V, Nb, Ta, Cr, Mo, W, Ni, Al, Si, and P are all small but have an effect of reducing the coercive force. However, if the addition exceeds 7%, the saturation magnetic flux density decreases, so the upper limit was made 7%.
以下、本発明について実施例によって具体的に説明する。
通常、垂直磁気記録媒体における軟磁性膜層は、その成分と同じ成分のスパッタリングターゲット材をスパッタし、ガラス基板などの上に成膜し得られる。ここでスパッタにより成膜された薄膜は急冷されている。これに対し、本発明では実施例、比較例の供試材として、単ロール式の液体急冷装置にて作製した急冷薄帯を用いている。これは実際にスパッタにより急冷され成膜された薄膜の、成分による諸特性への影響を、簡易的に液体急冷薄帯により評価したものである。
Hereinafter, the present invention will be specifically described with reference to examples.
Usually, a soft magnetic film layer in a perpendicular magnetic recording medium can be formed on a glass substrate or the like by sputtering a sputtering target material having the same component. Here, the thin film formed by sputtering is rapidly cooled. On the other hand, in this invention, the quenching thin strip produced with the single roll type liquid quenching apparatus is used as a test material of an Example and a comparative example. This is a simple evaluation of the influence of the components on various properties of a thin film formed by quenching by sputtering in a simple manner using a liquid quenching ribbon.
急冷薄帯の作業条件としては、表１の成分に秤量した原料３０ｇを径１０ｍｍ、高さ４０ｍｍ程度の水冷銅鋳型にて減圧Ａｒ中でアーク溶解し、急冷薄帯の溶解母材とした。急冷薄帯の作製条件は、単ロール方式で、径１５ｍｍの石英管中にこの溶解母材にセットし、出湯ノズル径を１ｍｍとし、雰囲気圧６１ｋＰａ、噴霧差圧６９ｋＰａ、銅ロール（径３００ｍｍ）の回転数３０００ｒｐｍ、銅ロールと出湯ノズルのギャップ０．３ｍｍにて出湯した。また、溶解母材の溶け落ち直後に出湯した。このようにして作製した急冷薄帯を供試材とし、以下の項目を評価した。 As the working conditions for the quenched ribbon, 30 g of the raw materials weighed in the components shown in Table 1 were arc-melted in reduced pressure Ar using a water-cooled copper mold having a diameter of about 10 mm and a height of about 40 mm to obtain a quenched preform. The conditions for preparing the quenched ribbon are the single roll method, set in this molten base material in a quartz tube with a diameter of 15 mm, the tap nozzle diameter is 1 mm, the atmospheric pressure is 61 kPa, the spray differential pressure is 69 kPa, and the copper roll (diameter is 300 mm) The hot water was discharged at a rotation speed of 3000 rpm and a gap between the copper roll and the hot water nozzle of 0.3 mm. Moreover, the hot water was poured out immediately after the molten base material melted down. The following items were evaluated using the thus prepared quenched ribbon as a test material.
急冷薄帯の保磁力の評価としては、振動試料型の保磁力メータにて、試料台に両面テープで急冷リボンを貼り付け、初期印加磁場１４４ｋＡ／ｍにて測定した。保磁力が５０Ａ／ｍ以下を○、５０Ａ／ｍを超え１００Ａ／ｍ以下を△、１００Ａ／ｍを超えるものを×とした。 For the evaluation of the coercive force of the rapidly cooled ribbon, a vibration sample type coercive force meter was used, and a quenching ribbon was affixed to the sample stage with a double-sided tape, and the initial applied magnetic field was 144 kA / m. A coercive force of 50 A / m or less was evaluated as ◯, a value exceeding 50 A / m and 100 A / m or less as Δ, and a value exceeding 100 A / m as ×.
急冷薄帯の飽和磁束密度の評価としては、ＶＳＭ装置（振動試料型磁力計）にて、印加磁場１２００ｋＡ／ｍで測定した。供試材の重量は１５ｍｇ程度。０．５Ｔ以上を○、０．５Ｔ未満を×として評価した。 As the evaluation of the saturation magnetic flux density of the quenched ribbon, it was measured with an applied magnetic field of 1200 kA / m with a VSM apparatus (vibrating sample magnetometer). The weight of the test material is about 15 mg. The evaluation was evaluated as O for 0.5T or more and x for less than 0.5T.
急冷薄帯の非晶質性の評価としては、通常、非晶質材料のＸ線回折パターンを測定すると、回折ピークが見られず、非晶質特有のハローパターンとなる。また、完全な非晶質でない場合は、回折ピークは見られるものの、結晶材料と比較しピーク高さが低くなり、かつ、ハローパターンも見られる。そこで、下記の方法にて非晶質性を評価した。 As an evaluation of the amorphous property of the quenched ribbon, usually, when an X-ray diffraction pattern of an amorphous material is measured, a diffraction peak is not seen and a halo pattern peculiar to an amorphous state is obtained. Moreover, when it is not completely amorphous, although a diffraction peak is seen, a peak height becomes low compared with a crystalline material, and a halo pattern is also seen. Therefore, amorphousness was evaluated by the following method.
ガラス板に両面テープで供試材を貼り付け、Ｘ線回折装置にて回折パターンを得た。このとき、測定面は急冷薄帯の銅ロール接触面となるように供試材をガラス板に貼り付けた。Ｘ線源はＣｕ−Ｋα線で、スキャンスピード４°／ｍｉｎで測定した。この回折パターンにハローパターンが確認できるものを○、全くハローパターンが見られないものを×として非晶質性の評価とした。 The test material was attached to a glass plate with a double-sided tape, and a diffraction pattern was obtained with an X-ray diffractometer. At this time, the test material was affixed on the glass plate so that the measurement surface was a copper roll contact surface of a quenched ribbon. The X-ray source was Cu—Kα ray, and measurement was performed at a scan speed of 4 ° / min. In this diffraction pattern, the evaluation of the amorphous property was evaluated as ◯ when the halo pattern could be confirmed, and x when no halo pattern was observed.
急冷薄帯の耐食性の評価としては、ガラス板に両面テープで供試材を貼り付け、５％ＮａＣｌの食塩水で、温度が３５℃、噴霧時間１６時間の条件の下で塩水噴霧試験を行い、全面発銹したものは×、一部発銹したものは○として評価した。また、急冷薄帯のビッカース硬度の評価としては、急冷リボンを縦に樹脂埋め研磨し、ビッカース硬度計にて測定した。測定荷重は５０ｇで１０点測定しその平均で評価した。８００ＨＶ以上を○、８００ＨＶ未満を×とした。圧痕のサイズは１０μｍ程度であった。 To evaluate the corrosion resistance of the quenched ribbon, a specimen was attached to a glass plate with double-sided tape, and a salt spray test was performed with 5% NaCl saline at a temperature of 35 ° C and a spraying time of 16 hours. The case where the entire surface was found was evaluated as x, and the case where a part was found was evaluated as ○. Moreover, as evaluation of the Vickers hardness of a quenching ribbon, the quenching ribbon was vertically resin-filled and polished, and measured with a Vickers hardness meter. The measurement load was measured at 10 points at 50 g, and the average was evaluated. 800 HV or more was rated as ◯, and less than 800 HV as x. The size of the indentation was about 10 μm.
表１および表２に示すように、比較例Ｎｏ．１２は、成分組成であるＨｆ含有量が低いために、保磁力の値が高く、かつ十分な非晶質性が得られない。比較例Ｎｏ．１３は、成分組成であるＺｒとＨｆの合計含有量が高く、かつ成分組成に係る式（１）の２×（Ｚｒ％＋Ｈｆ％）−Ｂの値が高いために、保磁力の値が高く、かつ飽和磁束密度が劣る。比較例Ｎｏ．１４は、成分組成に係る式（１）の２×（Ｚｒ％＋Ｈｆ％）−Ｂの値が高いために、保磁力が劣る。 As shown in Tables 1 and 2, Comparative Example No. No. 12 has a low coercive force value due to a low Hf content as a component composition, and a sufficient amorphous property cannot be obtained. Comparative Example No. No. 13 has a high total coercivity because the total content of the component composition Zr and Hf is high and the value of 2 × (Zr% + Hf%) − B of the formula (1) relating to the component composition is high. In addition, the saturation magnetic flux density is inferior. Comparative Example No. No. 14 is inferior in coercive force because the value of 2 × (Zr% + Hf%) − B in the formula (1) relating to the component composition is high.
比較例Ｎｏ．１５は、成分組成に係る式（１）の２×（Ｚｒ％＋Ｈｆ％）−Ｂの値が低いために、保磁力が劣る。比較例Ｎｏ．１６は、成分組成であるＢが含有量しないために、保磁力の悪く、かつ十分な非晶質性が得られないし、硬度が低い。比較例Ｎｏ．１７は、成分組成であるＢの含有量が高いために、飽和磁束密度が悪い。比較例Ｎｏ．１８は、成分組成に係る式（２）のＦｅ％（Ｆｅ％＋Ｃｏ％）の値が高いために、保磁力が悪い。比較例Ｎｏ．１９は、成分組成であるＮｂとＰの合計量が高いために、飽和磁束密度が悪い。 Comparative Example No. No. 15 is inferior in coercive force because the value of 2 × (Zr% + Hf%) − B in the formula (1) relating to the component composition is low. Comparative Example No. No. 16 does not contain B which is a component composition, so that the coercive force is poor and sufficient amorphousness cannot be obtained and the hardness is low. Comparative Example No. No. 17 has a low saturation magnetic flux density due to a high content of B as a component composition. Comparative Example No. No. 18 has a low coercive force because of the high value of Fe% (Fe% + Co%) in the formula (2) relating to the component composition. Comparative Example No. No. 19 has a low saturation magnetic flux density because the total amount of Nb and P which are component compositions is high.
これに対し、本発明例であるＮｏ．１〜１１は、いずれも本発明の条件を満足していることから、飽和磁束密度、非晶質性、耐食性、硬度なる各性能について優れていることが分かる。ただ、本発明例Ｎｏ．１、２、５、６、８〜１２は、保磁力がやや劣るが、しかし全体的には優れた性能を有する。 On the other hand, No. which is an example of the invention. Nos. 1 to 11 satisfy the conditions of the present invention, so that it can be seen that the performances of saturation magnetic flux density, amorphousness, corrosion resistance, and hardness are excellent. However, Invention Example No. 1, 2, 5, 6, 8 to 12 have slightly poor coercive force, but overall have excellent performance.
次に、スパッタリングターゲット材の製造方法の例を示す。Ｎｏ．５の組成に秤量した溶解原料を、減圧Ａｒガス雰囲気の耐火物坩堝内で誘導加熱溶解した後、坩堝下部の直径８ｍｍのノズルより出湯し、Ａｒガスによりアトマイズした。このガスアトマイス粉末を原料粉末として、炭素鋼製の直径２５０ｍｍ、長さ１００ｍｍのカプセル内に充填、真空脱気封入した。この粉末充填ビレットを、成形温度１０００℃、成形圧力１４７ＭＰａ、成形時間５時間の条件でＨＩＰ成形した。このＨＩＰ体から、機械加工により直径１８０ｍｍ、厚さ７ｍｍのスパッタリングターゲット材を作製した。このスパッタリングターゲット材は割れや欠けもなく製造可能であった。 Next, the example of the manufacturing method of sputtering target material is shown. No. The melted raw material weighed to the composition of No. 5 was induction-heated and melted in a refractory crucible in a reduced pressure Ar gas atmosphere, then poured out from a nozzle having a diameter of 8 mm at the bottom of the crucible and atomized with Ar gas. This gas atomized powder was used as a raw material powder, filled into a carbon steel capsule having a diameter of 250 mm and a length of 100 mm, and vacuum deaerated and sealed. This powder-filled billet was HIP molded under the conditions of a molding temperature of 1000 ° C., a molding pressure of 147 MPa, and a molding time of 5 hours. A sputtering target material having a diameter of 180 mm and a thickness of 7 mm was produced from this HIP body by machining. This sputtering target material could be manufactured without cracking or chipping.
以上のように、本発明により低い保磁力、高非晶質性、高耐食性および高硬度を有する垂直磁気記録媒体用軟磁性合金およびこの合金の薄膜を作製するためのスパッタリングターゲットを提供することが出来る極めて優れた効果を奏するものである。
特許出願人 山陽特殊製鋼株式会社
代理人 弁理士 椎 名 彊
As described above, the present invention provides a soft magnetic alloy for perpendicular magnetic recording media having low coercive force, high amorphousness, high corrosion resistance and high hardness, and a sputtering target for producing a thin film of this alloy. An extremely excellent effect that can be achieved.
Patent Applicant Sanyo Special Steel Co., Ltd.
Attorney: Attorney Shiina
Claims (5)
６≦２×（Ｚｒ％＋Ｈｆ％）−Ｂ％≦１６ … （１） at. %, One or two of Zr and Hf in total 6 to 20%, B 1 to 20%, the balance being Co and inevitable impurities, and satisfying the formula (1) Soft magnetic alloy for recording media.
6 ≦ 2 × (Zr% + Hf%) − B% ≦ 16 (1)
Ｆｅ％／（Ｆｅ％＋Ｃｏ％）＜０．２０ … （２） The soft magnetic alloy for magnetic recording media according to claim 1, wherein Fe is added, and the added amount satisfies the formula (2).
Fe% / (Fe% + Co%) <0.20 (2)
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| JP2010186876A JP5631659B2 (en) | 2010-08-24 | 2010-08-24 | Soft magnetic alloy and sputtering target material for perpendicular magnetic recording medium, and magnetic recording medium |
| MYPI2013700286A MY162173A (en) | 2010-08-24 | 2011-08-19 | Soft magnetic alloy for perpendicular magnetic recording medium, sputtering target material, and magnetic recording medium |
| PCT/JP2011/068790 WO2012026405A1 (en) | 2010-08-24 | 2011-08-19 | Soft magnetic alloy for magnetic recording medium, sputtering target material, and magnetic recording medium |
| SG2013012620A SG188252A1 (en) | 2010-08-24 | 2011-08-19 | Soft magnetic alloy for magnetic recording medium, sputtering target material, and magnetic recording medium |
| CN201180040330.8A CN103098135B (en) | 2010-08-24 | 2011-08-19 | Magnetic recording media non-retentive alloy, sputtering target material and magnetic recording media |
| US13/817,645 US9208812B2 (en) | 2010-08-24 | 2011-08-19 | Soft magnetic alloy for magnetic recording medium, sputtering target material, and magnetic recording medium |
| TW100130281A TWI480383B (en) | 2010-08-24 | 2011-08-24 | A magneto-optical recording medium for a magnetic recording medium, a sputtering target material, and a magnetic recording medium |
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| US20140090751A1 (en) * | 2012-10-03 | 2014-04-03 | Ut-Battelle, Llc | Hf-Co-B Alloys as Permanent Magnet Materials |
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| US9824711B1 (en) * | 2014-02-14 | 2017-11-21 | WD Media, LLC | Soft underlayer for heat assisted magnetic recording media |
| JP6405261B2 (en) * | 2014-05-01 | 2018-10-17 | 山陽特殊製鋼株式会社 | Soft magnetic alloy for magnetic recording, sputtering target material, and magnetic recording medium |
| JP2017057490A (en) * | 2015-09-18 | 2017-03-23 | 山陽特殊製鋼株式会社 | Co-Fe-B based alloy target material |
| JP6660130B2 (en) | 2015-09-18 | 2020-03-04 | 山陽特殊製鋼株式会社 | CoFeB alloy target material |
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- 2011-08-19 CN CN201180040330.8A patent/CN103098135B/en not_active Expired - Fee Related
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| CN103098135A (en) | 2013-05-08 |
| TW201219577A (en) | 2012-05-16 |
| US9208812B2 (en) | 2015-12-08 |
| WO2012026405A1 (en) | 2012-03-01 |
| US20130224067A1 (en) | 2013-08-29 |
| TWI480383B (en) | 2015-04-11 |
| CN103098135B (en) | 2016-01-20 |
| MY162173A (en) | 2017-05-31 |
| JP5631659B2 (en) | 2014-11-26 |
| SG188252A1 (en) | 2013-04-30 |
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